柱前衍生–高效液相色谱法测定肉类中氰化物含量的研究
A Study on the Determination of Cyanide in Meat by Pre-Column Derivatization-High Performance Liquid Chromatography
DOI: 10.12677/hjfns.2025.146092, PDF,   
作者: 吴余欣, 黄 南, 钟世欢, 项睿洁, 叶佳明, 王 京, 潘雷明*:浙江公正检验中心有限公司,浙江 杭州;蒋 晗:中国计量大学生命科学学院,浙江 杭州;王馨远:杭州市食品药品检验科学研究院食品检验研究所,浙江 杭州
关键词: 氰化物高效液相色谱法异烟酸–吡唑啉酮柱前衍生Cyanide HPLC Isonicotinic Acid-Pyrazoline Pre-Column Derivatization
摘要: 建立柱前衍生–高效液相色谱法测定肉类中氰化物含量的检测方法。样品经水蒸气蒸馏,采用异烟酸–吡唑啉酮柱前衍生,高效液相色谱法测定。采用迪马Silversil C18 (4.6 mm × 250 mm, 5 μm)色谱柱,以0.02 mol/L乙酸铵–甲醇(65:35)为流动相。检测波长638 nm。氰化物的衍生产物在0.02~110 mg/kg这一浓度范围里线性状况良好,其相关系数超过0.999,检出限为0.02 mg/kg。猪肉、鸭肉、狗肉中氰化物的平均回收率均大于95%。
Abstract: A method for determining the cyanide content in meat using pre-column derivatization-high-performance liquid chromatography was established. The sample was subjected to steam distillation, and the pre-column derivatization was performed using isonicotinic acid-pyrazoline. The cyanide derivative was determined by high-performance liquid chromatography. The Silversil C18 (4.6 mm × 250 mm, 5 μm) column from Dima was used, and the mobile phase was acetate ammonium-methanol (65:35). The detection wavelength was 638 nm. The linear relationship was good within the concentration range of 0.02~110 mg/kg, with a correlation coefficient of over 0.999. The detection limit was 0.02 mg/kg. The average recovery rates of cyanide in pork, duck, and dog meat were all greater than 95%.
文章引用:吴余欣, 黄南, 钟世欢, 项睿洁, 叶佳明, 王京, 蒋晗, 王馨远, 潘雷明. 柱前衍生–高效液相色谱法测定肉类中氰化物含量的研究[J]. 食品与营养科学, 2025, 14(6): 837-845. https://doi.org/10.12677/hjfns.2025.146092

参考文献

[1] Leavesley, H.B., Li, L., Prabhakaran, K., Borowitz, J.L. and Isom, G.E. (2007) Interaction of Cyanide and Nitric Oxide with Cytochrome C Oxidase: Implications for Acute Cyanide Toxicity. Toxicological Sciences, 101, 101-111. [Google Scholar] [CrossRef] [PubMed]
[2] Nelson, L. (2006) Acute Cyanide Toxicity: Mechanisms and Manifestations. Journal of Emergency Nursing, 32, S8-S11. [Google Scholar] [CrossRef] [PubMed]
[3] 郭忠, 张文德. 食品中的氰化物来源及其安全性的研究进展[J]. 中国食品卫生杂志, 2014, 26(4): 404-408.
[4] 袁宝君, 郑云雁, 谢华民, 等. GB5009.36-2023食品安全国家标准食品中氰化物的测定[S]. 北京: 中国标准出版社, 2023.
[5] 张侗琳, 屈海英, 徐德江, 等. 流动注射-分光光度法测量总氰化物的研究[J]. 山东化工, 2023, 52(2): 132-134.
[6] 常迪, 徐克赞, 赵立晶, 等. 全自动流动注射分析仪快速测定白酒中微量氰化物[J]. 酿酒科技, 2024(5): 139-144.
[7] 董娇, 骆德丽, 何云霄, 等. 白酒中氰化物含量测定方法优化[J]. 中国酒, 2024(11): 32-33.
[8] 宋逸群, 孙倩倩. 食品中氰化物检验方法的研究进展[J]. 福建分析测试, 2021, 30(3): 14-17.
[9] 祖新, 杨玲娟, 李羽翡, 等. 氰化物检测技术研究进展[J]. 工业水处理, 2020, 40(3): 11-16.
[10] 左家信, 范翔, 李欣, 等. 顶空-气相色谱法测定饮用水中的氰化物和氯化氰[J]. 分析仪器, 2023(5): 36-40.
[11] 邸玉敏, 朱军, 常靖, 等. 氰化物检测方法研究进展[J]. 理化检验(化学分册), 2011, 47(12): 1491-1494.
[12] 何维为, 徐灿辉, 何超, 等. 柱前衍生-高效液相色谱法测定酒中的氰化物[J]. 食品与药品, 2021, 23(2): 128-132.